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CAS No. : | 1877-72-1 | MDL No. : | MFCD00002486 |
Formula : | C8H5NO2 | Boiling Point : | - |
Linear Structure Formula : | (NC)(C6H4)COOH | InChI Key : | GYLKKXHEIIFTJH-UHFFFAOYSA-N |
M.W : | 147.13 | Pubchem ID : | 15875 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H315-H319-H335 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
62% | With sulfuric acid; for 12h;Reflux; | To a stirred solution of 3-cyanobenzoic acid (XXVII; 6 g; 41 mmol) in methanol (80 mL) was added catalytic sulfuric acid (5 mL). The reaction mixture was heated to a reflux for 12 hours. The reaction mixture was cooled, concentrated under reduced pressure and diluted with water.The aqueous layer was extracted with ethyl acetate (3 x 50 mL). The combined organic layers were washed with sodium bicarbonate, brine, dried over Na2SO4, filtered and concentrated under vacuum to afford methyl 3-cyanobenzoate as a white solid (XXVIII; 3 g, 62percent yield). ?H NMR (400 MHz, CDC13): oe 8.36 (s, 1H), 8.26-8.24 (d, J = 8.0 Hz, 1H), 7.84-7.82 (d, J = 8.0 Hz, 1H), 7.63-7.58 (m 1H), 3.95 (s, 3H). |
Preparation H11: Synthesis of 3-(thiazol-2-yl)benzoic Acid Preparation H11, Step 1: 10 g (0.068 mol) of 3-cyano benzoic acid was taken in 150 ml of dry dichloromethane and cooled to 0° C. Added 50 ml of oxalyl chloride drop wise followed by 5 drops of dry DMF. The reaction mixture was stirred at RT overnight. Dichloromethane was removed and dry methanol (50 ml) was added and stirred at rt for 2 h. Excess methanol was removed and the residue was dissolved in ethyl acetate. The ethyl acetate layer was washed with 10percent of sodium bicarbonate, brine and concentrated to give methyl 3-cyanobenzoate (7 g) as a white solid. | ||
11.5 g | With sulfuric acid; In toluene; at 70 - 100℃; for 5h; | 10.0 g (0.068 mol) of 3-cyanobenzoic acid, 20 ml of toluene, 20 g (0.625 mol) of methanol and 0.4 g (0.004 mol) of concentrated sulfuric acid were placed in a reaction vessel and stirred for 5 hours while dehydrating at an internal temperature of 70 to 100 ° C. . The reaction solution was cooled and water was added to separate the solution. The organic layer was concentrated under reduced pressure to obtain 11.5 g of a white solid. Next, the whole amount of the obtained white solid was placed in a reaction vessel and dissolved in 40 ml of methanol, and 5.3 g (0.076 mol) of hydroxylamine hydrochloride was added thereto. 8.1 g (0.078 mol) of triethylamine was added and the mixture was stirred at 30 to 40 ° C. for 2 hours. The reaction solution was cooled, 8.1 g (0.079 mol) of acetic anhydride was added, and the mixture was further stirred for 30 minutes. After completion of the reaction, the reaction solution was cooled and placed in a pressure-resistant container, 0.67 g of 10percent palladium carbon catalyst and 0.34 g of water were added and reacted under a hydrogen pressure of 0.3 Mpa for 4 hours. The catalyst was separated by filtration and washed with methanol to obtain the desired methanol solution. |
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